CN102275915B - Preparation method of high specific surface area scalar porous active carbon material - Google Patents

Preparation method of high specific surface area scalar porous active carbon material Download PDF

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CN102275915B
CN102275915B CN201110143990.0A CN201110143990A CN102275915B CN 102275915 B CN102275915 B CN 102275915B CN 201110143990 A CN201110143990 A CN 201110143990A CN 102275915 B CN102275915 B CN 102275915B
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陆安慧
李文翠
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Dalian University of Technology
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Abstract

The invention relates to a preparation method of a high specific surface area scalar porous active carbon material. The preparation method comprises the following steps: treating an SiO2 loaded core carbonized material as an activator, aging, cleaning, drying, activating, and removing SiO2 with an alkali or hydrofluoric acid or ammonium fluoride. In the preparation method provided by the invention, the core carbonized material is dipped with a sodium silicate or tetraethyl orthosilicate solution to load SiO2 as the activator, and is activated by vapor to prepare the active carbon material which has a balanced mesopore-micropore ratio. The active carbon with the scalar and porous structure can improve the filter effect of the material to harmful substances in vapor phase relative to micropore active carbon, is suitable for the filed of gas-liquid phase adsorption and separation, and can be applied to electrode materials of super capacitors or carriers of catalysts, and the scalar porous active carbon with prosper mesopores has a higher reproducibility than core-based microporous active carbon reported before.

Description

A kind of preparation method of high-ratio surface integral level porous activated carbon material
Technical field
The present invention relates to a kind of preparation method of high specific surface area granular activated carbon material, relate in particular to and a kind ofly take hard fruit shell as raw material, the effectively synthetic method with macropore, mesoporous and micropore graded pore structural gac.
Background technology
Active carbon with high specific surface area has vesicular structure, can adsorb various organism and inorganics, has the advantages that loading capacity is large, rate of adsorption is fast, is a kind of high-efficiency adsorbent of high-quality, is widely used in the every field such as foodstuffs industry, chemical industry and environment protection.
The starting material of composite reactive charcoal generally include shell (coconut husk, nut-shell, apricot shell, Nux Canarii albi, apple core etc.), wood chip, peat, bone, coal tar, synthetic resins and related polymer.The shell of hard has good natural structure, is the good material of preparing gac.And shell, with its cheapness, easily obtains and is conducive to the advantage of environment sustainable development and receives great concern.The application of active fruit shell carbon material is very extensive, comprises that the purification of refining decolouring, water and air of vegetables oil and chemical solvents is, the recovery of the recovery of solvent, precious metal, gas filter and face guard etc.
The absorption property of absorbent charcoal material depends on physics and the chemical property of material, comprises the specific surface area of particle shape, size, pore size, material and surface functional group etc.Wherein the specific surface area of gac, pore size and distribution thereof are the key factors that determines its adsorptive power.While only having aperture size to be about to be adsorbed 2 times of molecule critical diameter above, could there is active adsorption.
The method of industrial common employing carbonization-activation is prepared gac.Conventional activated media comprises carbonic acid gas, water vapor, phosphoric acid, potassium hydroxide, zinc chloride etc., although the gac specific surface area obtaining is high, micropore be take as main in aperture.When adsorption molecule is larger, be difficult to enter in the micropore of gac.When particularly flow velocity is very fast, the utilization ratio of micropore will decline greatly.For the absorption property of enhanced activity charcoal, in the urgent need to preparation, be rich in the gac of meso-hole structure.
Shell is widely used in the preparation of absorbent charcoal material, US2005221981-A1 as a kind of natural matter; US7799733-B2, employing Exocarpium cocois (Cocos nucifera L) is raw material, and zinc chloride, potassium hydroxide etc. is activator, and obtaining aperture is the micropore gac of 1.7～2.1nm.But active fruit shell carbon prepared by this method exists regenerative power low, microporosity is high, and activator is to problems such as equipment corrosions.For overcoming these problems, can adopt the method for carbonizing polymer and synthetic resins to prepare gac, although this class absorbent charcoal material microstructure has good controllability, but their preparation cost is far away higher than active fruit shell carbon.Therefore, how developing a cost-effective preparation method, to obtain the absorbent charcoal material that pore structure is controlled, specific surface area is high, absorption property is strong be current urgent problem.
Summary of the invention
The object of the present invention is to provide a kind of novel method of synthetic graduation porous active Carbon Materials, take fruit shell carbon material as raw material, SiO 2for activator, through load SiO 2, aging, clean, dry, steam activation and alkali cleaning remove SiO 2etc. step, prepare targeted activity Carbon Materials; Described method is as follows:
Fruit shell carbon material is immersed in the solution of silicon source with load SiO 2, SiO 2theoretical negative carrying capacity be 1%～40%, optimum load amount is 2%～15%; According to theoretical negative carrying capacity, calculate the concentration of silicon source solution, configuration silicon source solution.Described silicon source solution is tetraethyl orthosilicate solution or sodium silicate solution.
In the present invention, fruit shell carbon material is immersed in the solution of silicon source, under air-proof condition, in 10 ℃～60 ℃, place 5～72h with load activator SiO 2.
To above-mentioned load SiO 2fruit shell carbon material carry out aging: to being soaked with in the silicon source solution of fruit shell carbon material, add concentrated hydrochloric acid, stir, in room temperature lower seal, place 1～4h, then in 50 ℃～90 ℃ seal aging 12～36h.The present invention's concentrated hydrochloric acid used is commercially available concentrated hydrochloric acid commodity (mass concentrations 36～37%), its consumption and SiO 2mol ratio be 0.4-40.
Fruit shell carbon material after aging is cleaned to neutrality repeatedly with deionized water, to remove because of load SiO 2, the operation such as aging remains in the chemical substance in fruit shell carbon material, avoids it to affect follow-up reactivation process.Purging method can adopt suction filtration, and dried overnight is postactivated at 80 ℃.
Thereby the activation of absorbent charcoal material is by the duct in material and the process that caves in and open or expand the material of acquisition bigger serface.The method of activation has a lot, and relatively more conventional is physically activated or chemical activation at present.The present invention adopts physical activation method, by the steam activation 30min～4h under 700 ℃～1100 ℃ nitrogen protections of the fruit shell carbon material after cleaning-drying.The temperature of reactivation process is controlled very important, if temperature is too low, priming reaction is slow, lacks economy; If temperature is too high, reaction is by diffusion control, and this will cause the loss of raw material.Therefore, steam activation 1～2h under preferably 800 ℃～1000 ℃ nitrogen protections of the present invention.Certainly, the present invention also can adopt chemical activation method, for example, adopts KOH or ZnCl 2activated material; But chemical activation method may cause disadvantageous chemical substance deposition and equipment corrosion in Carbon Materials, although the chemical substance of these depositions can be by thoroughly washing removal, but comparatively speaking, physical activation method operation is more simple and convenient, and economy can be handling strong.
Gac after activation removes SiO with alkaline solution washing 2.Also can adopt hydrofluoric acid, Neutral ammonium fluoride to remove the SiO on gac 2.That considers process safety and technique can be handling, uses alkaline solution, and as alkali obtain solutions such as sodium hydroxide, potassium hydroxide, its concentration and consumption are on net result of the present invention without impact, and the object of alkaline solution washing is only to remove the SiO of load on gac 2.
In the present invention, shell load SiO 2need first to carry out charing: natural shell is carried out to charing in 400～800 ℃ of pyrolysis 1～24h, then by pulverizing, reduce shell and be of a size of follow-up load SiO before 2larger surface-area is provided; After pulverization process, screening granular size is that 5 order～80 object powder are used as fruit shell carbon material of the present invention, preferred 10 order～60 orders, and optimum range is 20 order～40 orders.Shell of the present invention comprises nut, nutshell, as Pistacia vera, nut-shell or coconut husk etc., and the rejected material of other fruit, as almond, palm core and olive waste material etc.; Because shell all consists of lignocellulose, its soft or hard degree ratio of Mierocrystalline cellulose and xylogen in lignocellulose decides, and in other words, any material that comprises vast scale lignocellulose or hard lignin material are all applicable to being applied to the present invention.
Particle size: the absorbent charcoal material of preparing by the inventive method, can control particle size according to the demand of application, the particle size after initial shell crushing and screening can reduce 10%～40%.But absorbent charcoal material particle is unsuitable too small, in order to avoid method centrifugal by tradition or that filter is difficult to reclaim sorbent material in fractionation by adsorption use procedure.On the other hand, as excessive in fruit granule, the specific surface area of unit volume material can reduce, thereby causes the decline of adsorption efficiency.Therefore, to prepare the optimal size reduction amount of absorbent charcoal material be 15%～25% to the inventive method.Consider above-mentioned factor, the gac that uses the inventive method to prepare has 10 μ m～4000 μ m median sizes, and median size should be at 50 μ m～2000 μ m preferably.
Specific surface area: absorbent charcoal material specific surface area is to use nitrogen adsorption method to measure, nitrogen adsorption method is to measure the volume of material absorption nitrogen and the transformation relation of nitrogen balance dividing potential drop under steady temperature, utilize Brunauer, the mathematics model analysis result of Emmett and Teller invention obtains the method for specific surface area value, i.e. BET specific surface area.The specific surface area of absorbent charcoal material prepared by the inventive method is at least 1000m 2/ g, is at least 1200m preferably 2/ g.The specific surface area of absorbent charcoal material prepared by the inventive method is generally 1400,1450,1500,1550,1600,1650,1700,1750,1800,1850,1900,1950, or 2000m 2more than/g; Porous carbon material specific surface area is at 1500m preferably 2/ g～2100m 2/ g, the specific surface area of optimum porous carbon material is 1600m 2/ g～2000m 2/ g.
Vesicularity: in absorbent charcoal material, macropore, relative volume mesoporous and micropore can be measured by well-known nitrogen adsorption method and mercury penetration method.Mercury penetration method can be measured mesoporous and pore volume macropore, and nitrogen adsorption method can be used to measure micropore and mesoporous pore volume.Yet, because the theoretical foundation of these two kinds of methods is different, the pore volume that therefore can not directly relatively use two kinds of methods to measure.The absorbent charcoal material that the inventive method obtains has macropore, mesoporous and micropore graded pore structural, and wherein 40%～90% pore volume is provided by mesoporous.Conventionally this per-cent that specially the mesoporous minimum aperture volume of absorbent charcoal material in invention accounts in mesoporous, micropore and total pore volume is 45%, 55% and 65%, is conventionally 65%, 75% and 85% to the maximum.Preferably mesoporous volume averaging accounts for 45%～85% of mesoporous, micropore and total pore volume.The pore volume of porous carbon material prepared by the inventive method (measurement of nitrogen adsorption method) is at least 0.4cm 3/ g, can also reach 0.5,0.6,0.7,0.8,0.9 or 1.0cm 3/ g.It should be noted that Carbon Materials pore volume may cause the decline of density of material too greatly, affects the loadings of unit volume.
Density: pore passage structure and the density of material of absorbent charcoal material are closely bound up.Generally, the pore volume of material is larger, and density of material is less.Absorbent charcoal material prepared by the present invention has the 0.25g/cm of being greater than 3volume density, be greater than preferably 0.3g/cm 3, can also be greater than 0.5g/cm 3, 0.6g/cm 3or 0.7g/cm 3.Material true density prepared by the present invention is greater than 0.4g/cm 3, be greater than preferably 0.45g/cm 3, can also be greater than 0.55g/cm 3, 0.60g/cm 3or 0.65g/cm 3.
In sum, advantage of the present invention has been to provide a kind of method of novel synthesizing high specific surface area graduation porous active Carbon Materials.Fruit shell carbon material process dipping water glass or tetraethyl orthosilicate solution in the present invention, then the absorbent charcoal material of preparing after steam activation has balanced mesoporous and micropore ratio.This gac with graded porous structure is with respect to micropore gac, can improve the filter effect of material to gas phase objectionable impurities, be applicable to gas, liquid absorption and separation field, and this graduation porous activated carbon has higher recyclability than the micropore gac based on shell of reporting before this.
Another advantage of the present invention has been to provide a kind of method that adopts cheap natural materials and minimal steps composite reactive Carbon Materials, and uses existing or simple technique and instrument just can realize.
Consistent with those skilled in the art's prescriptive procedure to the definition of pore size in specification sheets of the present invention and claims, be about to the duct that aperture is less than 2nm and be defined as micropore, 2nm-50nm duct is defined as mesoporous, and aperture is greater than 50nm and is defined as macropore.
Accompanying drawing explanation
Fig. 1 is cyclic voltammetry curve (a) and the constant current charge-discharge curve (b) of the activated carbon sample prepared of the embodiment of the present invention.
Embodiment
Embodiment of the present invention can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
In the present invention, silicon source strength of solution is calculated by formula (1) method:
W % = m SiO 2 m C = C · V · m C · M SiO 2 m C × 100 % = ( C · V · M SiO 2 ) × 100 % - - - ( 1 )
Wherein, W%---silicon-dioxide is born theoretical carrying capacity;
M siO2---the silicon-dioxide quality of load, g;
M c---the quality of fruit shell carbon material, g;
C---the concentration of silicon source solution, mol/L;
V---the pore volume of fruit shell carbon material, cm 3/ g;
M siO2---SiO 2molecular weight, 60.08g/mol.
Concentrated hydrochloric acid consumption calculates by formula (2) method:
V = m C · W % · a · M HCl M SiO 2 · 37 % · ρ HCl - - - ( 2 )
Wherein, m c---the quality of fruit shell carbon material, g;
W%---silicon-dioxide is born theoretical carrying capacity;
A---hydrochloric acid and SiO 2mol ratio;
M hCl---the molecular weight of HCl, 36.5g/mol;
M siO2---SiO 2molecular weight, 60.08g/mol;
37%---the massfraction of hydrochloric acid;
ρ hCl---the density of 37% hydrochloric acid, 1.16g/mL.
Embodiment 1
Absorbent charcoal material sample F 1, according to the inventive method, take nut-shell as raw material, by carbonized material load SiO 2preparation.
Calculate the concentration of silicon source solution: take the fruit shell carbon material 1g of 600 ℃ of charings, physisorphtion is tested this fruit shell carbon material pore volume V=0.277cm 3/ g, wish is prepared SiO 2charge capacity is 1.88% raw material:
W % = m SiO 2 m C = C · V · m C · M SiO 2 m C = C × 0.277 × 10 - 3 × 1 × 60.08 1 × 100 % = 1.88 % ,
Calculate thus the concentration C of silicon source solution (with SiO 2meter) be 1.122mol/L.
Gac preparation: take natural nut-shell as raw material is in 600 ℃ of charing 4h, after pulverizing, get 20g active fruit shell carbon by SiO 2theoretical negative carrying capacity 1.88% is calculated, and uses the lower 10 ℃ of dipping 24h of 1.122mol/L sodium silicate solution air-proof condition; To above-mentioned steeping fluid, add the concentrated hydrochloric acid 4ml (add-on of concentrated hydrochloric acid is calculated and is about 4ml by formula (2)) of commercially available 37wt.% concentration, 4h is placed in room temperature sealing again, then in 50 ℃ of seal aging 24h; And then the cleaning of deionized water suction filtration is to neutral, is dried, at 850 ℃ of nitrogen protection steam activation 100min;
Getting concentration is the NaOH solution 160ml of 3.75mol/L, in 50 ℃ of product 24h that soak after activation, then with deionized water suction filtration, cleans to neutral 90 ℃ of dry nights.
The present embodiment has been prepared about 10g gac.
Embodiment 2
Absorbent charcoal material sample F 2, according to the inventive method, take coconut husk as raw material, by carbonized material load SiO 2preparation.
Take natural coconut husk as 800 ℃ of charing 2h of raw material, after pulverizing, press SiO 2theoretical negative carrying capacity 12.58% is calculated; use the lower 20 ℃ of dipping 1h of 4.402mol/L tetraethyl orthosilicate solution air-proof condition; in above-mentioned steeping fluid, add 37wt.% concentrated hydrochloric acid 300 μ L again; 2h is placed in room temperature sealing; 90 ℃ of seal aging 36h; deionized water suction filtration cleans to neutral again, is dried, then nitrogen protection steam activation 120min at 800 ℃.
Getting concentration is the alkaline solution 160ml of 3.75mol/L, in 50 ℃ of product 24h that soak after activation, then with deionized water suction filtration, cleans to neutral 90 ℃ of dry nights.
The present embodiment has been prepared about 10g gac.
Embodiment 3
Absorbent charcoal material sample F 3, according to the inventive method, take coconut husk as raw material, by carbonized material load SiO 2preparation.
Take natural coconut husk as 800 ℃ of charing 1h of raw material, after pulverizing, press SiO 2theoretical negative carrying capacity 2.72% is calculated; use the lower 20 ℃ of dipping 24h dippings of 1.074mol/L sodium silicate solution air-proof condition; in above-mentioned steeping fluid, add 37wt.% concentrated hydrochloric acid 800 μ L again; 1h is placed in room temperature sealing; 70 ℃ of seal aging 12h; deionized water suction filtration cleans to neutral again, is dried, then nitrogen protection steam activation 100min at 900 ℃.
Getting concentration is the alkaline solution 160ml of 3.75mol/L, in 50 ℃ of product 24h that soak after activation, then with deionized water suction filtration, cleans to neutral 90 ℃ of dry nights.
The present embodiment has been prepared about 10g gac.
Embodiment 4
Absorbent charcoal material sample F 4, according to the inventive method, take coconut husk as raw material, by carbonized material load SiO 2preparation.
Take natural coconut husk as 600 ℃ of charing 3h of raw material, after pulverizing, press SiO 2theoretical negative carrying capacity 2.70% is calculated; use the lower 50 ℃ of dipping 24h of 0.835mol/L sodium silicate solution air-proof condition; in above-mentioned steeping fluid, add 37wt.% concentrated hydrochloric acid 4ml again; 3h is placed in room temperature sealing; 50 ℃ of seal aging 12h; deionized water suction filtration cleans to neutral again, is dried, then nitrogen protection steam activation 60min at 1000 ℃.
Getting concentration is the alkaline solution 160ml of 3.75mol/L, in 50 ℃ of product 24h that soak after activation, then with deionized water suction filtration, cleans to neutral 90 ℃ of dry nights.
The present embodiment has been prepared about 10g gac.
Embodiment 5
Every physical properties to absorbent charcoal material sample F 1, F2, F3, F4 is tested.The characteristic parameter of absorbent charcoal material sample is as shown in table 1.Characteristic parameter comprises specific surface area (S bET), total pore volume (V total), the total pore volume (V of micropore micro) and non-Micropore volume (V other).
The present invention adopts Ecosorb CX experiment material in contrast, and Ecosorb CX is a kind of normal business gac of take the complete microvoid structure that coconut husk prepared as raw material steam activation.
Table 1 the inventive method is prepared the characteristic parameter of activated carbon sample
Figure GDA0000080885240000071
As can be seen from Table 1, the micro-porosity (V of sample F 1, F2, F3 and F4 micro/ V total) be all less than 50%, show wherein to contain a large amount of mesoporous.The micro-porosity of normal business gac Ecosorb CX is 100%, shows that hole is all comprised of micropore.
Activated carbon sample prepared by the embodiment of the present invention carries out the measurement of nitrogen adsorption method.Result shows, at relative pressure P/P 0< 0.2 place's adsorptive capacity has a fast rise, shows to be rich in sample micropore; At relative pressure P/P 0> 0.4 place, sample all has obvious hysteresis loop, shows to contain in sample abundant mesoporous.This illustrates that these absorbent charcoal materials have micropore and mesoporous graded pore structural.
Embodiment 6 does the electrochemical property test of electrode material for super capacitor
The absorbent charcoal material 45mg that gets embodiment 1 preparation, adds 8mg tetrafluoroethylene (PTFE) to make binding agent, and (sheet size is 1cm to be pressed into electrode slice 2).Take nickel foam as collector, in 6M KOH solution, take platinized platinum as supporting electrode, Hg/HgO is reference electrode, forms three electrode test systems of standard, carries out electrochemical property test.Electromotive force window setting range is :-0.8V～0V, and the scanning speed of cyclic voltammetry curve (CV) is chosen respectively 2mV/s, 5mV/s and 10mV/s, and the test current density of constant current charge-discharge curve (GC) is 2A/g.
As seen from Figure 1, the CV curve of electrode materials presents more regular rectangular characteristic (a), GC curve is isosceles triangle symmetrical (Fig. 1 b) to Fig. 1, and illustrative material has desirable electric double layer capacitance behavior.From GC curve, its volts lost is less as seen, and the internal resistance of illustrative material is lower, is applicable to doing electrode material for super capacitor.The capacitance of calculating under difference is swept speed with CV curve is respectively: 172F/g (2mV/s), 179F/g (5mV/s) and 175F/g (10mV/s).
Embodiment 7 adsorpting dye molecules (magenta) test
Get the absorbent charcoal material 0.04g of embodiment 3 preparations, the Basic Fuchsin in Aqueous Solution that adsorption concentration is 500mg/L, liquor capacity is 100mL, and adsorption temp is 20 ℃, and 400rpm stirs 24h, and equilibrium adsorption capacity is up to 796mg g -1.
Embodiment 8 CO absorption 2aptitude tests
The absorbent charcoal material 0.1g that gets embodiment 4 preparations, utilizes physical adsorption appearance ASAP 2020 in the time of 25 ℃, to carry out CO 2gas adsorption, adsorptive capacity can reach 2.14mmol/g (47.9cm 3/ g).
In sum, load SiO 2the absorbent charcoal material obtaining has abundant micropore and mesoporous graded pore structural, can be applicable to gas-liquid fractionation by adsorption field, such as the purification of solvent refined decolouring, water and air, the recovery of precious metal, gas filter and face guard, electrode material for super capacitor etc.

Claims (6)

1. a preparation method for high-ratio surface integral level porous activated carbon material, is characterized in that: fruit shell carbon material is immersed in the solution of silicon source, under air-proof condition, place 5～72h for 10 ℃～60 ℃, with load SiO 2as activator;
Described silicon source solution is tetraethyl orthosilicate solution or sodium silicate solution;
Described activation condition is 700 ℃～1100 ℃ nitrogen/steam activation 30min～4h; Gac after activation is removed SiO with alkaline solution washing 2, or remove the SiO on gac with hydrofluoric acid, Neutral ammonium fluoride 2.
2. the preparation method of high-ratio surface integral level porous activated carbon material according to claim 1, is characterized in that: described SiO 2theoretical negative carrying capacity be 1%～40%.
3. according to the preparation method of high-ratio surface integral level porous activated carbon material described in claim 1 or 2, it is characterized in that: by load SiO 2fruit shell carbon material immerse in concentrated hydrochloric acid, sealing is placed after 1～4h, in 50 ℃～90 ℃ aging 12～36h.
4. the preparation method of high-ratio surface integral level porous activated carbon material according to claim 3, is characterized in that: described concentrated hydrochloric acid consumption and SiO 2mol ratio be 0.4～40.
5. according to the preparation method of high-ratio surface integral level porous activated carbon material described in claim 1 or 2, it is characterized in that: activation condition is 800 ℃～1000 ℃ nitrogen/steam activation 1～2h.
6. according to the preparation method of high-ratio surface integral level porous activated carbon material described in claim 1 or 2, it is characterized in that: fruit shell carbon material is that natural shell carries out charing in 400 ℃～800 ℃ pyrolysis 1～24h, then through pulverizing, screen 5 order～80 object particles.
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CN103420371A (en) * 2013-08-06 2013-12-04 山东大学 Technological method for preparing reed activated carbon from potassium silicate as activator
CN103464104B (en) * 2013-10-08 2014-11-26 滁州华伦装饰材料有限公司 Active carbon and preparing method thereof
CN103971948A (en) * 2014-05-14 2014-08-06 山东理工大学 Method for preparing super capacitor carbon electrode material by using pistachio nut shell as raw materials
CN104556029B (en) * 2014-12-21 2017-03-08 沈阳工程学院 Petroleum residual oil is combined with tar slag and prepares activated carbon and fuel oil
CN106847524A (en) * 2016-12-16 2017-06-13 吴中区穹窿山师匠新材料技术咨询服务部 A kind of preparation method of activated carbon/silica/graphene complex
CN107628597B (en) * 2017-10-16 2020-04-28 河南师范大学 By using SiO2Method for preparing biomass carbon material with micropore and mesopore structure by coating method
CN108726576B (en) * 2018-06-01 2019-08-23 东莞理工学院 The continuous preparation porous charcoal/Fe of carbonization-activation oxidation3O4Method
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CN110559988A (en) * 2019-04-26 2019-12-13 福建工程学院 preparation method of activated carbon with strong adsorption
CN110354803B (en) * 2019-07-10 2021-06-08 大连理工大学 Integral composite porous carbon adsorption material for separating methane and nitrogen and preparation method thereof
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